HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58124888, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 58124938 | HCID 58124938 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Solvent | Sodium Acetate | HCID 517045 | — |
| Product | HCID 58124888 | HCID 58124888 | 22.1% |
Reaction Steps
A solution of 350 mg of 24g in 5 ml of acetic anhydride and 300 mg of sodium acetate, was heated at 90-100° C. for 3 h. The reaction was cooled to rt and 10 ml of water was added and stirring at ambient temperature was prolonged for 1 hr. The mixture was neutralized by addition of cold conc. NH4OH and the product was extracted with ethyl acetate. The organic extract was washed with water, dried and concentrated, and the remainders chromatographed over silicagel (using a gradient of heptane/ethyl acetate as eluent), to give 70 mg 24h (white crystalline material, triturated with heptane); Mp 175-177° C. Rf (heptane/ethyl acetate 1/1) 0.75.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08431564B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-457774a286dd4336babe42af7958b131 |
| Source note | uspto-grants-2013_04 |